CN115008851A - 一种高密度聚乙烯复合薄膜及其加工工艺 - Google Patents
一种高密度聚乙烯复合薄膜及其加工工艺 Download PDFInfo
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- CN115008851A CN115008851A CN202210766139.1A CN202210766139A CN115008851A CN 115008851 A CN115008851 A CN 115008851A CN 202210766139 A CN202210766139 A CN 202210766139A CN 115008851 A CN115008851 A CN 115008851A
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- density polyethylene
- polystyrene
- composite film
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 69
- 239000000203 mixture Substances 0.000 claims abstract description 60
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- 238000002844 melting Methods 0.000 claims abstract description 28
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- DLYUQMMRRRQYAE-UHFFFAOYSA-N tetraphosphorus decaoxide Chemical compound O1P(O2)(=O)OP3(=O)OP1(=O)OP2(=O)O3 DLYUQMMRRRQYAE-UHFFFAOYSA-N 0.000 claims description 36
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 claims description 34
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Classifications
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Abstract
本发明公开了一种高密度聚乙烯复合薄膜及其加工工艺,包括以下工艺:(1)备料:取高密度聚乙烯、聚苯乙烯、马来酸酐改性纳米二氧化硅、致孔剂、助剂,得到混合料A;取聚乙烯醇、改性聚苯乙烯、乙酸丁酯,得到混合料B;取高密度聚乙烯、聚苯乙烯、苯乙烯改性介孔二氧化硅、致孔剂、助剂,得到混合料C;(2)制备:取上述混合料A、混合料B、混合料C,分别熔融,共挤,依次形成增强层、亲水层、微孔层,得到复合薄。本发明通过对增强层、亲水层、微孔层孔径的控制,实现空气、水气在复合薄膜的单向流通;同时通过对增强层、亲水层、微孔层组分的配置,使得所制复合薄膜在具有优秀力学性能、透光性能的同时,提高防雾、阻隔性能。
Description
技术领域
本发明涉及复合薄膜技术领域,具体为一种高密度聚乙烯复合薄膜及其加工工艺。
背景技术
在常见的防护用品中,透明阻隔膜能够杜绝飞沫传染,将顾客、服务人员、商品在物理空间上隔离开来,切断病毒空气传播途径,为顾客、服务人员等提供安全无忧消费环境。而受湿度和温度的影响,水蒸气常在阻隔膜上凝结,对顾客、服务人员的视野造成妨碍。因此,我们提出一种高密度聚乙烯复合薄膜及其加工工艺。
发明内容
本发明的目的在于提供一种高密度聚乙烯复合薄膜及其加工工艺,以解决上述背景技术中提出的问题。
为了解决上述技术问题,本发明提供如下技术方案:一种高密度聚乙烯复合薄膜的加工工艺,包括以下工艺:
(1)备料:
取高密度聚乙烯、聚苯乙烯、马来酸酐改性纳米二氧化硅、致孔剂、助剂,得到混合料A;
取聚乙烯醇、改性聚苯乙烯、乙酸丁酯,得到混合料B;
取高密度聚乙烯、聚苯乙烯、苯乙烯改性介孔二氧化硅、致孔剂、助剂,得到混合料C;
(2)制备:
取上述混合料A、混合料B、混合料C,分别熔融,共挤,依次形成增强层、亲水层、微孔层,得到复合薄膜。
进一步的,所述增强层的孔径小于亲水层的孔径,所述亲水层的孔径小于微孔层的孔径。
进一步的,所述增强层的平均孔径为20~40nm,亲水层的平均孔径为60~80nm,微孔层的平均孔径为100~120nm。
进一步的,所述复合薄膜的厚度为25~100μm。
进一步的,包括以下工艺:
(1)备料:
取高密度聚乙烯、聚苯乙烯、马来酸酐改性纳米二氧化硅、致孔剂、助剂,180~210℃熔融混合1~2h,得到混合料A;
取聚乙烯醇、改性聚苯乙烯、乙酸丁酯,230~250℃熔融,回流混合1~2h,得到混合料B;
取高密度聚乙烯、聚苯乙烯、苯乙烯改性介孔二氧化硅、致孔剂、助剂,180~210℃熔融混合1~2h,得到混合料C;
(2)制备:
将上述熔融的混合料A、混合料B、混合料C,同步挤入具有三层结构的流延机模头中,流延挤出并牵引成膜,模头温度为200~220℃;依次形成增强层、亲水层、微孔层,进行热处理,热处理工艺为100~120℃退火50~60min,得到复合薄膜。
进一步的,所述增强层包括以下重量组分:60~70份高密度聚乙烯、25~30份聚苯乙烯、7~10份马来酸酐改性纳米二氧化硅、3~6份致孔剂、0.6~1.5份助剂。
进一步的,所述亲水层包括以下重量组分:60~67份聚乙烯醇、30~33份改性聚苯乙烯、30~45份聚乙烯吡咯烷酮。
进一步的,所述微孔层包括以下重量组分:60~70份高密度聚乙烯、25~30份改性聚苯乙烯、7~10份苯乙烯改性介孔二氧化硅、10~15份致孔剂、0.6~1.5份助剂。
进一步的,助剂为0.1~0.5份抗氧剂164、0.4~0.9份紫外线吸收剂UV-531、0.1~0.3份防老剂264;致孔剂为聚乙烯吡咯烷酮。
在上述技术方案中,增强层作为对外膜层,亲水层作为芯层,微孔层作为对内膜层,其孔径依次增大;在所制复合膜层薄膜使用时,由外至内逐渐增大的孔隙使得复合薄膜内的空气、水气加速向外流通,而较小的外层孔隙使得向内的空气、水气流通减少,促进水气、空气向外的单向流通,在透气、透湿的同时,所制复合薄膜能够提高对外界阻隔性能,保持内部的干燥、清洁;
其中,增强层选择高密度聚乙烯、聚苯乙烯、马来酸酐改性纳米二氧化硅作为共混基体,高密度聚乙烯、聚苯乙烯的二元有机体系,使得所制增强层具有优秀的力学性能和透光性能,加入的马来酸酐改性纳米二氧化硅在改善透光性能、力学性能的同时,也对二者的相容性进行改善,得到具有高透光、高强度的增强层;
亲水层由聚乙烯醇、改性聚苯乙烯、聚乙烯吡咯烷酮共混制得,其中聚乙烯吡咯烷酮、聚乙烯醇间形成氢键,相容性好使得所制亲水层的结晶度下降,亲水性能提高,提高亲水层对水气的吸附,增加水气在亲水层中的扩散,促进水气向外输送,并能够提高透光性、水气通量,避免水气在复合薄膜内的凝集,防止水气对所制复合薄膜透光率造成负面影响,赋予其防雾性能;聚乙烯醇与改性聚苯乙烯交联,提高了亲水层的稳定性,溶剂在亲水层吸附、扩散的协同效应得到限制,使得亲水层对通过的溶剂进行选择,减少除水气外的挥发性能物质外溢与进入,提高所制复合薄膜的阻隔性能;通过控制亲水层的熔融混合、挤出温度,使得体系中的聚乙烯吡咯烷酮部分溢出,得到具有孔隙的亲水层,与增强层、微孔层配合;
微孔层由高密度聚乙烯、改性聚苯乙烯、苯乙烯改性介孔二氧化硅组成,介孔二氧化硅具有较高的粗糙度,利于水气的吸附,所制微孔层与亲水层间的界面结合能力提高,并在提高所制微孔层力学性能的同时,提高其透光率;而苯乙烯对介孔二氧化硅的改性,能够在改善透光率的同时,提高其与高密度聚乙烯、改性聚苯乙烯间的相容性;苯乙烯改性介孔二氧化硅的具体改性步骤为:取丙酮,加入二氧化硅、KH570、马来酸酐,在氮气氛围下,加热搅拌回流3h,得到马来酸酐改性二氧化硅;然后在氮气氛围中,过氧化苯甲酰的引发作用下,与苯乙烯,加热反应3h。
进一步的,所述改性聚苯乙烯的制备包括以下工艺:
(1)单体的合成:
取四氢呋喃,在氮气氛围中,加入4,4’-二羟基二环己烷、三乙胺,冰浴条件下,滴加丙烯酰氯,室温反应24~36h;加入甲醇,旋蒸,洗涤,干燥,得到单酯A;
取丙酮,加入环状磷酸酐,加热至60~65℃,搅拌溶解,缓慢滴加蒸馏水,反应100~150min,过滤,50~60℃干燥24h,得到水解产物B;
取水解产物B,加入单酯A、阳离子树脂,95~105℃反应4.6~5.4h,过滤,无水乙醇洗涤,取下层滤液,旋蒸,得到单体;
(2)超支化聚苯乙烯的合成:
在氩气无氧条件下,取乙烯基苄基氯溶于氯苯,冷冻除氧,得到乙烯基苄基氯溶液;取氯化亚铜、2’2-联吡啶溶于氯苯,冷冻除氧,得到铜盐溶液A;
取乙烯基苄基氯溶液,加入铜盐溶液A,升温至115~125℃,搅拌反应3.7~4.3h;于液氮猝冷,加入四氢呋喃,过中性氧化铝柱,旋蒸浓缩,加入甲醇,取沉淀干燥,得到超支化聚苯乙烯;
(3)改性聚苯乙烯的合成:
在氩气无氧条件下,取溴化亚铜、五甲基二乙烯三胺,加入除氧后的苯甲醚,配置得到铜盐溶液B;取苯甲醚,加入超支化聚苯乙烯、单体,配置成单体溶液;
将铜盐溶液B加入到单体溶液中,搅拌均匀,置于85~95℃温度下,搅拌加热2.7~3.3h;于液氮猝冷,通入空气,加入四氢呋喃稀释,过中性氧化铝柱以除去铜盐,旋蒸浓缩,加入甲醇,过滤,干燥,得到改性聚苯乙烯。
进一步的,所述(1)中4,4’-二羟基二环己烷、丙烯酰氯、三乙胺的摩尔比为1:(1.1~1.5):(1.7~2.5)。
进一步的,所述环状磷酸酐、丙酮的质量比为(0.5~0.6):1。
进一步的,所述环状磷酸酐水解产物、单酯A、阳离子树脂的比例为(0.17~0.18)mol:(0.17~0.20)mol:(3.5~3.6)g。
进一步的,所述乙烯基苄基氯、氯苯的体积比为3:(8.2~8.6)。
进一步的,所述乙烯基苄基氯、氯化亚铜、2,2-联吡啶的摩尔比为(21.0~21.5):(2.0~2.2):(4.3~4.5)。
进一步的,所述溴化亚铜、五甲基二乙烯三胺的摩尔比为1:(1.08~1.10)。
进一步的,所述超支化聚苯乙烯、苯甲醚的质量比为(9.0~9.3):1。
进一步的,超支化聚苯乙烯、单体、溴化亚铜、五甲基二乙烯三胺的质量比为(30~45):(72.5~75.0):(0.10~0.11):(0.14~0.15)。
在上述技术方案中,4,4’-二羟基二环己烷中的羟基与丙烯酰氯中的酰氯反应,通过控制4,4’-二羟基二环己烷、丙烯酰氯、三乙胺的摩尔比——1:(1.1~1.5):(1.7~2.5),和反应的后处理工艺,得到含有二环己烷、羟基的单酯A;环状磷酸酐水解,在阳离子树脂的催化下与单酯A中未反应的羟基反应,得到单体;然后以乙烯基苄基氯为单体,氯化亚铜、2’2-联吡啶为铜盐催化,以氯苯为溶剂,发生原子转移自由基自缩聚反应,制备超支化的含氯聚苯乙烯,记为超支化聚苯乙烯;因其带有大量的氯原子,能够作为大分子引发剂引发单体的聚合,以溴化亚铜、五甲基二乙烯三胺为铜盐催化,发生原子转移自由基聚合反应,引发上述所制单体的聚合,得到改性聚苯乙烯;
将上述所制改性聚苯乙烯引入聚乙烯醇体系中,改性聚苯乙烯中的O=P-OH能够与聚乙烯醇的-OH发生反应,提高交联度,降低聚乙烯醇的结晶性,提高其透光性的同时,改善所制亲水膜的强度和柔韧性。由上述制备工艺,改性聚苯乙烯形成了超支化结构,能够降低熔体粘度,提高混合料B的加工性能,改善亲水层的力学性能;同时聚合物中引入的磷、氮,能够形成磷酸作为脱水剂,促进聚合物成炭,形成保护层,降低热传导,阻止热量和物质传递;可吸热,阻止氧化反应的进程;赋予所制复合隔膜优秀的阻燃性能,改善其热稳定性;
与现有技术相比,本发明的有益效果如下:
1.本发明的高密度聚乙烯复合薄膜及其加工工艺,通过对增强层、亲水层、微孔层孔径的控制,促进所制复合薄膜的单向流通,加速空气、水气向外流通;同时通过对增强层、亲水层、微孔层组分的配置,使得所制复合薄膜在具有优秀力学性能、透光性能的同时,提高防雾、阻隔性能。
2.本发明的高密度聚乙烯复合薄膜及其加工工艺,通过4,4’-二羟基二环己烷、丙烯酰氯、环状磷酸酐制备聚合单体,将其与乙烯基苄基氯制得的超支化聚苯乙烯接枝,得到改性聚苯乙烯,将其加入亲水层、微孔层组分体系中,能够提高其力学性能、透光性能,并改善其相容性、加工性能。
具体实施方式
下面将对本发明实施例中的技术方案进行清楚完整地描述,显然,所描述的实施例仅仅是本发明一部分实施例,而不是全部的实施例。基于本发明中的实施例,本领域普通技术人员在没有做出创造性劳动前提下所获得的所有其他实施例,都属于本发明保护的范围。
实施例1
(1)备料:
1.1.改性聚苯乙烯的制备:
(1.1.1)单体的合成:
取四氢呋喃,在氮气氛围中,加入4,4’-二羟基二环己烷、三乙胺、氯化铝,冰浴条件下,滴加丙烯酰氯,室温反应24h;加入甲醇,旋蒸,洗涤,干燥,得到单酯A;
取丙酮,加入环状磷酸酐,加热至60℃,搅拌溶解,缓慢滴加蒸馏水,反应100min,过滤,50℃干燥24h,得到水解产物B;
取水解产物B,加入单酯A、阳离子树脂,95℃反应4.6h,过滤,无水乙醇洗涤,取下层滤液,旋蒸,得到单体;
(1.1.2)超支化聚苯乙烯的合成:
在氩气无氧条件下,取乙烯基苄基氯溶于氯苯,冷冻除氧,得到乙烯基苄基氯溶液;取氯化亚铜、2’2-联吡啶溶于氯苯,冷冻除氧,得到铜盐溶液A;
取乙烯基苄基氯溶液,加入铜盐溶液A,升温至115℃,搅拌反应3.7h;于液氮猝冷,加入四氢呋喃,过中性氧化铝柱,旋蒸浓缩,加入甲醇,取沉淀干燥,得到超支化聚苯乙烯;
(1.1.3)改性聚苯乙烯的合成:
在氩气无氧条件下,取溴化亚铜、五甲基二乙烯三胺,加入除氧后的苯甲醚,配置得到铜盐溶液B;取苯甲醚,加入超支化聚苯乙烯、单体,配置成单体溶液;
将铜盐溶液B加入到单体溶液中,搅拌均匀,置于85℃温度下,搅拌加热2.7h;于液氮猝冷,通入空气,加入四氢呋喃稀释,过中性氧化铝柱以除去铜盐,旋蒸浓缩,加入甲醇,过滤,干燥,得到改性聚苯乙烯;
4,4’-二羟基二环己烷、丙烯酰氯、三乙胺的摩尔比为1:1.1:1.7;环状磷酸酐、丙酮的质量比为0.5:1;环状磷酸酐水解产物、单酯A、阳离子树脂的比例为0.17mol:0.17mol:3.5g;乙烯基苄基氯、氯苯的体积比为3:8.2;乙烯基苄基氯、氯化亚铜、2,2-联吡啶的摩尔比为21.0:2.0:4.3;溴化亚铜、五甲基二乙烯三胺的摩尔比为1:1.08;超支化聚苯乙烯、单体、溴化亚铜、五甲基二乙烯三胺的质量比为30:72.5:0.10:0.14;
1.2.取60份高密度聚乙烯、25份聚苯乙烯、7份马来酸酐改性纳米二氧化硅、3份致孔剂、0.6份助剂,180℃熔融混合1h,得到混合料A;
取60份聚乙烯醇、30份改性聚苯乙烯、30份聚乙烯吡咯烷酮,230℃熔融,回流混合1h,得到混合料B;
取60份高密度聚乙烯、25份改性聚苯乙烯、7份苯乙烯改性介孔二氧化硅、10份致孔剂、0.6份助剂,180℃熔融混合1h,得到混合料C;
助剂为0.1份抗氧剂164、0.4份紫外线吸收剂UV-531、0.1份防老剂264;致孔剂为聚乙烯吡咯烷酮;上述份数均为重量组分;
(2)制备:
将上述熔融的混合料A、混合料B、混合料C,同步挤入具有三层结构的流延机模头中,流延挤出并牵引成膜,模头温度为200℃;依次形成增强层、亲水层、微孔层,进行热处理,热处理工艺为100℃退火50min,得到复合薄膜;
增强层的平均孔径为20nm,亲水层的平均孔径为60nm,微孔层的平均孔径为100nm;复合薄膜的厚度为25μm。
实施例2
(1)备料:
1.1.改性聚苯乙烯的制备:
(1.1.1)单体的合成:
取四氢呋喃,在氮气氛围中,加入4,4’-二羟基二环己烷、三乙胺、氯化铝,冰浴条件下,滴加丙烯酰氯,室温反应30h;加入甲醇,旋蒸,洗涤,干燥,得到单酯A;
取丙酮,加入环状磷酸酐,加热至62℃,搅拌溶解,缓慢滴加蒸馏水,反应120min,过滤,55℃干燥24h,得到水解产物B;
取水解产物B,加入单酯A、阳离子树脂,100℃反应5h,过滤,无水乙醇洗涤,取下层滤液,旋蒸,得到单体;
(1.1.2)超支化聚苯乙烯的合成:
在氩气无氧条件下,取乙烯基苄基氯溶于氯苯,冷冻除氧,得到乙烯基苄基氯溶液;取氯化亚铜、2’2-联吡啶溶于氯苯,冷冻除氧,得到铜盐溶液A;
取乙烯基苄基氯溶液,加入铜盐溶液A,升温至120℃,搅拌反应4h;于液氮猝冷,加入四氢呋喃,过中性氧化铝柱,旋蒸浓缩,加入甲醇,取沉淀干燥,得到超支化聚苯乙烯;
(1.1.3)改性聚苯乙烯的合成:
在氩气无氧条件下,取溴化亚铜、五甲基二乙烯三胺,加入除氧后的苯甲醚,配置得到铜盐溶液B;取苯甲醚,加入超支化聚苯乙烯、单体,配置成单体溶液;
将铜盐溶液B加入到单体溶液中,搅拌均匀,置于90℃温度下,搅拌加热3h;于液氮猝冷,通入空气,加入四氢呋喃稀释,过中性氧化铝柱以除去铜盐,旋蒸浓缩,加入甲醇,过滤,干燥,得到改性聚苯乙烯;
4,4’-二羟基二环己烷、丙烯酰氯、三乙胺的摩尔比为1:1.3:2.0;环状磷酸酐、丙酮的质量比为0.55:1;环状磷酸酐水解产物、单酯A、阳离子树脂的比例为0.17mol:0.18mol:3.6g;乙烯基苄基氯、氯苯的体积比为3:8.4;乙烯基苄基氯、氯化亚铜、2,2-联吡啶的摩尔比为21.3:2.1:4.4;溴化亚铜、五甲基二乙烯三胺的摩尔比为1:1.09;超支化聚苯乙烯、苯甲醚的质量比为9.2:1;超支化聚苯乙烯、单体、溴化亚铜、五甲基二乙烯三胺的质量比为38:73.8:0.105:0.145;
1.2.取65份高密度聚乙烯、27份聚苯乙烯、8份马来酸酐改性纳米二氧化硅、5份致孔剂、1.0份助剂,190℃熔融混合1.5h,得到混合料A;
取64份聚乙烯醇、32份改性聚苯乙烯、38份聚乙烯吡咯烷酮,240℃熔融,回流混合1.5h,得到混合料B;
取65份高密度聚乙烯、28份改性聚苯乙烯、9份苯乙烯改性介孔二氧化硅、12份致孔剂、1.0份助剂,195℃熔融混合1.5h,得到混合料C;
助剂为0.3份抗氧剂164、0.5份紫外线吸收剂UV-531、0.2份防老剂264;致孔剂为聚乙烯吡咯烷酮;上述份数均为重量组分;
(2)制备:
将上述熔融的混合料A、混合料B、混合料C,同步挤入具有三层结构的流延机模头中,流延挤出并牵引成膜,模头温度为210℃;依次形成增强层、亲水层、微孔层,进行热处理,热处理工艺为110℃退火55min,得到复合薄膜;
增强层的平均孔径为30nm,亲水层的平均孔径为70nm,微孔层的平均孔径为110nm;复合薄膜的厚度为25μm
实施例3
(1)备料:
1.1.改性聚苯乙烯的制备:
(1.1.1)单体的合成:
取四氢呋喃,在氮气氛围中,加入4,4’-二羟基二环己烷、三乙胺、氯化铝,冰浴条件下,滴加丙烯酰氯,室温反应36h;加入甲醇,旋蒸,洗涤,干燥,得到单酯A;
取丙酮,加入环状磷酸酐,加热至65℃,搅拌溶解,缓慢滴加蒸馏水,反应150min,过滤,60℃干燥24h,得到水解产物B;
取水解产物B,加入单酯A、阳离子树脂,105℃反应5.4h,过滤,无水乙醇洗涤,取下层滤液,旋蒸,得到单体;
(1.1.2)超支化聚苯乙烯的合成:
在氩气无氧条件下,取乙烯基苄基氯溶于氯苯,冷冻除氧,得到乙烯基苄基氯溶液;取氯化亚铜、2’2-联吡啶溶于氯苯,冷冻除氧,得到铜盐溶液A;
取乙烯基苄基氯溶液,加入铜盐溶液A,升温至125℃,搅拌反应4.3h;于液氮猝冷,加入四氢呋喃,过中性氧化铝柱,旋蒸浓缩,加入甲醇,取沉淀干燥,得到超支化聚苯乙烯;
(1.1.3)改性聚苯乙烯的合成:
在氩气无氧条件下,取溴化亚铜、五甲基二乙烯三胺,加入除氧后的苯甲醚,配置得到铜盐溶液B;取苯甲醚,加入超支化聚苯乙烯、单体,配置成单体溶液;
将铜盐溶液B加入到单体溶液中,搅拌均匀,置于95℃温度下,搅拌加热3.3h;于液氮猝冷,通入空气,加入四氢呋喃稀释,过中性氧化铝柱以除去铜盐,旋蒸浓缩,加入甲醇,过滤,干燥,得到改性聚苯乙烯;
4,4’-二羟基二环己烷、丙烯酰氯、三乙胺的摩尔比为1:1.5:2.5;环状磷酸酐、丙酮的质量比为0.6:1;环状磷酸酐水解产物、单酯A、阳离子树脂的比例为0.18mol:0.20mol:3.6g;乙烯基苄基氯、氯苯的体积比为3:8.6;乙烯基苄基氯、氯化亚铜、2,2-联吡啶的摩尔比为21.5:2.2:4.5;溴化亚铜、五甲基二乙烯三胺的摩尔比为1:1.10;超支化聚苯乙烯、苯甲醚的质量比为9.3:1;超支化聚苯乙烯、单体、溴化亚铜、五甲基二乙烯三胺的质量比为45:75.0:0.11:0.15;
1.2.取70份高密度聚乙烯、30份聚苯乙烯、10份马来酸酐改性纳米二氧化硅、6份致孔剂、1.5份助剂,210℃熔融混合2h,得到混合料A;
取67份聚乙烯醇、33份改性聚苯乙烯、45份聚乙烯吡咯烷酮,250℃熔融,回流混合2h,得到混合料B;
取70份高密度聚乙烯、30份改性聚苯乙烯、10份苯乙烯改性介孔二氧化硅、15份致孔剂、1.5份助剂,210℃熔融混合2h,得到混合料C;
助剂为0.4份抗氧剂164、0.8份紫外线吸收剂UV-531、0.3份防老剂264;致孔剂为聚乙烯吡咯烷酮;上述份数均为重量组分;
(2)制备:
将上述熔融的混合料A、混合料B、混合料C,同步挤入具有三层结构的流延机模头中,流延挤出并牵引成膜,模头温度为220℃;依次形成增强层、亲水层、微孔层,进行热处理,热处理工艺为120℃退火60min,得到复合薄膜;
增强层的平均孔径为40nm,亲水层的平均孔径为80nm,微孔层的平均孔径为100nm;复合薄膜的厚度为25μm。
对比例1
1.1.改性聚苯乙烯的制备:
(1.1.1)单体的合成:
取四氢呋喃,在氮气氛围中,加入4,4’-二羟基二环己烷、三乙胺、氯化铝,冰浴条件下,滴加丙烯酰氯,室温反应24h;加入甲醇,旋蒸,洗涤,干燥,得到单体;
步骤(1)其他步骤(1.1.2、1.1.3、1.2)、步骤(2)与实施例1相同,得到复合薄膜。
对比例2
1.1.改性聚苯乙烯的制备:
聚苯乙烯的合成:
在氩气无氧条件下,取苯乙烯溶于氯苯,冷冻除氧,得到苯乙烯溶液;取氯化亚铜、2’2-联吡啶溶于氯苯,冷冻除氧,得到铜盐溶液A;
取苯乙烯溶液,加入铜盐溶液A,升温至115℃,搅拌反应3.7h;于液氮猝冷,加入四氢呋喃,过中性氧化铝柱,旋蒸浓缩,加入甲醇,取沉淀干燥,得到改性苯乙烯。
步骤1.2、步骤(2)与实施例1相同,得到复合薄膜。
对比例3
1.2.取60份高密度聚乙烯、25份聚苯乙烯、7份KH570改性纳米二氧化硅、3份致孔剂、0.6份助剂,180℃熔融混合1h,得到混合料A;
取60份聚乙烯醇、30份改性聚苯乙烯、30份聚乙烯吡咯烷酮,210℃熔融,回流混合1h,得到混合料B;
取60份高密度聚乙烯、25份改性聚苯乙烯、7份KH570改性纳米二氧化硅、10份致孔剂、0.6份助剂,180℃熔融混合1h,得到混合料C;
助剂为0.1份抗氧剂164、0.4份紫外线吸收剂UV-531、0.1份防老剂264;致孔剂为聚乙烯吡咯烷酮;上述份数均为重量组分;
步骤1.1、步骤(2)与实施例1相同,得到复合薄膜。
对比例4
(1)备料:
取60份高密度聚乙烯、25份聚苯乙烯、7份KH570改性纳米二氧化硅、3份致孔剂、0.6份助剂,180℃熔融混合1h,得到混合料A;
取60份聚乙烯醇、30份聚苯乙烯、30份聚乙烯吡咯烷酮,210℃熔融,回流混合1h,得到混合料B;
取60份高密度聚乙烯、25份聚苯乙烯、7份KH570改性纳米二氧化硅、10份致孔剂、0.6份助剂,180℃熔融混合1h,得到混合料C;
助剂为0.1份抗氧剂164、0.4份紫外线吸收剂UV-531、0.1份防老剂264;致孔剂为聚乙烯吡咯烷酮;上述份数均为重量组分;
步骤(2)与实施例1相同,得到复合薄膜。
对比例5
(1)备料:
取60份高密度聚乙烯、7份KH570改性纳米二氧化硅、3份致孔剂、0.6份助剂,180℃熔融混合1h,得到混合料A;
取60份聚乙烯醇、30份聚乙烯吡咯烷酮,210℃熔融,回流混合1h,得到混合料B;
取60份高密度聚乙烯、7份KH570改性纳米二氧化硅、10份致孔剂、0.6份助剂,180℃熔融混合1h,得到混合料C;
助剂为0.1份抗氧剂164、0.4份紫外线吸收剂UV-531、0.1份防老剂264;致孔剂为聚乙烯吡咯烷酮;上述份数均为重量组分;
步骤(2)与实施例1相同,得到复合薄膜。
对比例6
(1)备料:
取60份高密度聚乙烯、7份KH570改性纳米二氧化硅、3份致孔剂、0.6份助剂,180℃熔融混合1h,得到混合料A;
取60份聚乙烯醇、6份聚乙烯吡咯烷酮,210℃熔融,回流混合1h,得到混合料B;
取60份高密度聚乙烯、7份KH570改性纳米二氧化硅、3份致孔剂、0.6份助剂,180℃熔融混合1h,得到混合料C;
助剂为0.1份抗氧剂164、0.4份紫外线吸收剂UV-531、0.1份防老剂264;致孔剂为聚乙烯吡咯烷酮;上述份数均为重量组分;
步骤(2)与实施例1相同,得到复合薄膜。
对比例7
(1)备料:
取60份高密度聚乙烯、7份KH570改性纳米二氧化硅、3份致孔剂、0.6份助剂,180℃熔融混合1h,得到混合料A;
取60份高密度聚乙烯、7份KH570改性纳米二氧化硅、3份致孔剂、0.6份助剂,180℃熔融混合1h,得到混合料C;
助剂为0.1份抗氧剂164、0.4份紫外线吸收剂UV-531、0.1份防老剂264;致孔剂为聚乙烯吡咯烷酮;上述份数均为重量组分;
(2)制备:
将上述熔融的混合料A、混合料C,同步挤入具有三层结构的流延机模头中,流延挤出并牵引成膜,模头温度为200℃;依次形成增强层、微孔层,进行热处理,热处理工艺为100℃退火50min,得到复合薄膜。
上述高密度聚乙烯:TR-144,购买于中国石油化工股份有限公司,熔体流动速率为0.18g/10min,密度为0.946g/cm3;
聚苯乙烯:PG33,购买于中国台湾奇美实业股份有限公司,熔体流动速率为8.5g/10min,洛氏硬度为M-76,维卡软化点为95℃;
聚乙烯吡咯烷酮:购买于上海阿拉丁生化科技股份有限公司;
聚乙烯醇:购买于上海阿拉丁生化科技股份有限公司,相对分子质量为105000;
环状磷酸酐为2-甲基-2,5-二氧磷杂环戊烷:购买于国药集团化学试剂有限公司;
KH570改性纳米二氧化硅:取0.4gKH570,加入0.3g去离子水,乙酸调节pH至3.5,水解2h,得到水解液;取1g纳米二氧化硅于300g甲苯中超声分散60min,升温至75℃,加入水解液,反应7.5h,得到KH570改性纳米二氧化硅;
马来酸酐改性纳米二氧化硅由以下工艺制得:取300g丙酮,加入200mgKH570改性纳米二氧化硅、5.0g马来酸酐、0.10g氧化苯甲酰,在氮气氛围下,加热至75℃反应3h,得到马来酸酐改性二氧化硅;
苯乙烯改性介孔二氧化硅由以下工艺制得:利用马来酸酐改性纳米二氧化硅的制备工艺制备马来酸酐改性介孔二氧化硅。在氮气氛围中,取300g丙酮,200mg马来酸酐改性介孔二氧化硅,加入0.08g过氧化苯甲酰、3.82g苯乙烯,加热至75℃反应3h。
致孔剂聚乙烯吡咯烷酮在增强层、亲水层、微孔层流延、牵伸成膜工艺中采用水浴浸渍萃取;
增强层、亲水层、微孔层平均孔径的测试方法:取50cm2圆片作为试样,采用循环水真空泵进行测试,在27MPa压力下,测得透过试样的纯水体积,平均孔径为r= ,为纯水粘度,△P为工作压力,A为试样有效面积,L为试样厚度,Q为纯水的体积流量,ℇ为试样孔隙率。
复合薄膜厚度的测试方法:采用扫描电子显微镜进行测试。
实验
取实施例1-3、对比例1-7中得到的复合薄膜,制得试样,分别对其性能进行检测并记录检测结果:
可见光透光率:采用紫外可见分光光度计,对试样的紫外可见光透过率进行测试,扫描范围400~800nm。
拉伸强度:以GB/T 13022为参考标准,试样尺寸150mm×50mm,拉伸速度5mm/min。
水气透过率:以GB/T 12704.1为参考标准,对试样的透湿量进行测试。
防雾性能:以GB/T 31726中的急速热雾法为参考标准,对试样的防雾性能进行测试。
根据上表中的数据,可以清楚得到以下结论:
实施例1-3中得到的复合薄膜与对比例1-7中得到的复合薄膜形成对比,检测结果可知,
1、与对比例7相比,实施例1-3中得到的复合薄膜,其透光率、拉伸强度、水气透过率、防雾性能实验数据较优,这充分说明了本申请实现了对所制复合薄膜力学性能、防雾性能、透光性能、水气透过性能的提高;
2、与实施例1相比,对比例1-6中得到的复合薄膜,其透光率、拉伸强度、水气透过率、防雾性能实验数据均有所劣化,且使用聚苯乙烯的对比例,其加工性能较差,熔体粘度较高,不利于所制复合薄膜的质量均一性能;可知本申请对,增强层、亲水层、微孔层三膜层组分及其制备工艺的设置,能够促进所制复合薄膜力学性能、防雾性能、透光性能、水气透过性能、加工性能的改善。
需要说明的是,在本文中,诸如第一和第二等之类的关系术语仅仅用来将一个实体或者操作与另一个实体或操作区分开来,而不一定要求或者暗示这些实体或操作之间存在任何这种实际的关系或者顺序。而且,术语“包括”“包含”或者其任何其他变体意在涵盖非排他性的包含,从而使得包括一系列要素的过程方法物品或者设备不仅包括那些要素,而且还包括没有明确列出的其他要素,或者是还包括为这种过程方法物品或者设备所固有的要素。
最后应说明的是:以上所述仅为本发明的优选实施例而已,并不用于限制本发明,尽管参照前述实施例对本发明进行了详细的说明,对于本领域的技术人员来说,其依然可以对前述各实施例所记载的技术方案进行修改,或者对其中部分技术特征进行等同替换。凡在本发明的精神和原则之内,所作的任何修改等同替换改进等,均应包含在本发明的保护范围之内。
Claims (10)
1.一种高密度聚乙烯复合薄膜的加工工艺,其特征在于:包括以下工艺:
(1)备料:
取高密度聚乙烯、聚苯乙烯、马来酸酐改性纳米二氧化硅、致孔剂、助剂,得到混合料A;
取聚乙烯醇、改性聚苯乙烯、乙酸丁酯,得到混合料B;
取高密度聚乙烯、聚苯乙烯、苯乙烯改性介孔二氧化硅、致孔剂、助剂,得到混合料C;
(2)制备:
取上述混合料A、混合料B、混合料C,分别熔融,共挤,依次形成增强层、亲水层、微孔层,得到复合薄膜。
2.根据权利要求1所述的一种高密度聚乙烯复合薄膜的加工工艺,其特征在于:所述改性聚苯乙烯的制备包括以下工艺:
(1)单体的合成:
取四氢呋喃,在氮气氛围中,加入4,4’-二羟基二环己烷、三乙胺,冰浴条件下,滴加丙烯酰氯,室温反应24~36h;加入甲醇,旋蒸,洗涤,干燥,得到单酯A;
取丙酮,加入环状磷酸酐,加热至60~65℃,搅拌溶解,缓慢滴加蒸馏水,反应100~150min,过滤,50~60℃干燥24h,得到水解产物B;
取水解产物B,加入单酯A、阳离子树脂,95~105℃反应4.6~5.4h,过滤,无水乙醇洗涤,取下层滤液,旋蒸,得到单体;
(2)超支化聚苯乙烯的合成:
在氩气无氧条件下,取乙烯基苄基氯溶于氯苯,冷冻除氧,得到乙烯基苄基氯溶液;取氯化亚铜、2’2-联吡啶溶于氯苯,冷冻除氧,得到铜盐溶液A;
取乙烯基苄基氯溶液,加入铜盐溶液A,升温至115~125℃,搅拌反应3.7~4.3h;于液氮猝冷,加入四氢呋喃,过中性氧化铝柱,旋蒸浓缩,加入甲醇,取沉淀干燥,得到超支化聚苯乙烯;
(3)改性聚苯乙烯的合成:
在氩气无氧条件下,取溴化亚铜、五甲基二乙烯三胺,加入除氧后的苯甲醚,配置得到铜盐溶液B;取苯甲醚,加入超支化聚苯乙烯、单体,配置成单体溶液;
将铜盐溶液B加入到单体溶液中,搅拌均匀,置于85~95℃温度下,搅拌加热2.7~3.3h;于液氮猝冷,通入空气,加入四氢呋喃稀释,过中性氧化铝柱以除去铜盐,旋蒸浓缩,加入甲醇,过滤,干燥,得到改性聚苯乙烯。
3.根据权利要求1所述的一种高密度聚乙烯复合薄膜的加工工艺,其特征在于:所述增强层的孔径小于亲水层的孔径,所述亲水层的孔径小于微孔层的孔径;
所述增强层的平均孔径为20~40nm,亲水层的平均孔径为60~80nm,微孔层的平均孔径为100~120nm。
4.根据权利要求1所述的一种高密度聚乙烯复合薄膜的加工工艺,其特征在于:所述增强层包括以下重量组分:60~70份高密度聚乙烯、25~30份聚苯乙烯、7~10份马来酸酐改性纳米二氧化硅、3~6份致孔剂、0.6~1.5份助剂。
5.根据权利要求1所述的一种高密度聚乙烯复合薄膜的加工工艺,其特征在于:所述亲水层包括以下重量组分:60~67份聚乙烯醇、30~33份改性聚苯乙烯、30~45份聚乙烯吡咯烷酮。
6.根据权利要求2所述的一种高密度聚乙烯复合薄膜的加工工艺,其特征在于:所述微孔层包括以下重量组分:60~70份高密度聚乙烯、25~30份改性聚苯乙烯、7~10份苯乙烯改性介孔二氧化硅、3~6份致孔剂、0.6~1.5份助剂。
7.根据权利要求2所述的一种高密度聚乙烯复合薄膜的加工工艺,其特征在于:所述(1)中4,4’-二羟基二环己烷、丙烯酰氯、三乙胺的摩尔比为1:(1.1~1.5):(1.7~2.5);所述环状磷酸酐、丙酮的质量比为(0.5~0.6):1;环状磷酸酐水解产物、单酯A、阳离子树脂的比例为(0.17~0.18)mol:(0.17~0.20)mol:(3.5~3.6)g。
8.根据权利要求2所述的一种高密度聚乙烯复合薄膜的加工工艺,其特征在于:所述乙烯基苄基氯、氯苯的体积比为3:(8.2~8.6);乙烯基苄基氯、氯化亚铜、2,2-联吡啶的摩尔比为(21.0~21.5):(2.0~2.2):(4.3~4.5)。
9.根据权利要求2所述的一种高密度聚乙烯复合薄膜的加工工艺,其特征在于:所述溴化亚铜、五甲基二乙烯三胺的摩尔比为1:(1.08~1.10);超支化聚苯乙烯、苯甲醚的质量比为(9.0~9.3):1;超支化聚苯乙烯、单体、溴化亚铜、五甲基二乙烯三胺的质量比为(30~45):(72.5~75.0):(0.10~0.11):(0.14~0.15)。
10.根据权利要求1-9任一项所述的加工工艺制得的一种高密度聚乙烯复合薄膜。
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